CN113308606B - Method for leaching and separating valuable metals from silver-gold-rich selenium steaming slag - Google Patents

Method for leaching and separating valuable metals from silver-gold-rich selenium steaming slag Download PDF

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CN113308606B
CN113308606B CN202110624239.6A CN202110624239A CN113308606B CN 113308606 B CN113308606 B CN 113308606B CN 202110624239 A CN202110624239 A CN 202110624239A CN 113308606 B CN113308606 B CN 113308606B
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selenium
leaching
tellurium
silver
copper
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CN113308606A (en
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徐宝强
甄甜甜
杨斌
蒋文龙
孔令鑫
田阳
王飞
刘大春
吴鉴
李一夫
熊恒
曲涛
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Kunming University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/007—Wet processes by acid leaching
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00—Obtaining noble metals
    • C22B11/04—Obtaining noble metals by wet processes
    • C22B11/042—Recovery of noble metals from waste materials
    • C22B11/044—Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B13/00—Obtaining lead
    • C22B13/04—Obtaining lead by wet processes
    • C22B13/045—Recovery from waste materials
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00—Obtaining copper
    • C22B15/0063—Hydrometallurgy
    • C22B15/0065—Leaching or slurrying
    • C22B15/0067—Leaching or slurrying with acids or salts thereof
    • C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Abstract

The invention discloses a method for leaching and separating valuable metals from silver-rich gold selenium steaming slag, and belongs to the fields of hydrometallurgy and secondary resource recycling. The method is characterized in that leaching is carried out in a sulfuric acid system in the presence of hydrogen peroxide and oxygen, solid-liquid separation is carried out after the reaction is finished, selenium, tellurium and copper are oxidized and enter an acidic leaching solution, and lead and noble metals are left in acidic leaching residues; the leaching rates of selenium, tellurium and copper under normal pressure reach 88.89%, 84.93% and 89.87%, respectively, and under the pressure condition reach 93.97%, 99.83% and 92.65%. The invention inhibits H by adding oxygen 2 O 2 The decomposition improves the leaching rate of selenium and tellurium, realizes the separation of selenium, tellurium and copper and noble metal, simultaneously reduces the intensity of reaction, and has simple process flow and convenient operation; the solution containing selenium, tellurium and copper obtained by separation is respectively used for recovering selenium, tellurium and copper by reduction, purification and the like; the slag containing the noble metal and the lead is sent to smelting for recovering the noble metal and the lead.

Description

Method for leaching and separating valuable metals from silver-gold-rich selenium steaming slag
Technical Field
The invention belongs to the field of hydrometallurgy and secondary resource recycling, and particularly relates to a method for leaching and separating valuable metals from silver-rich gold selenium steaming slag.
Background
Selenium and tellurium are important rare metals and are widely applied to the fields of metallurgy, materials, chemical industry, computers, agriculture, medical treatment and the like. In the crust, selenium is abundant only 5X 10 -8 Abundance of tellurium 6X 10 -8 And is difficult to realize large-scale industrial enrichment. At present, more than 90 percent of selenium and tellurium in the world are produced in the comprehensive treatment process of copper anode slime, and Ag is mainly used in the copper anode slime 2 Se、Cu 2 Se、CuAgSe、Cu 2 Te、Ag 2 Te、AuTe 2 The phase morphology of the equivalent exists. Copper anode slime is a smelting byproduct generated in the copper electrolytic refining process and is an important raw material for extracting noble metals (silver, gold and platinum group metals) and comprehensively recovering other valuable metals (selenium, tellurium and copper). During the recovery of valuable metals and purification of copper anode slime, slag rich in selenium, tellurium and noble metals is generated, and the slag becomes an important source for recovering rare and dispersed selenium and tellurium as well as gold, silver and platinum group metals.
The silver-rich gold selenium evaporation slag is crude selenium recovered from copper anode mud produced by copper smelting, and is subjected to a series of processes of closed smelting, vacuum distillation and the like to obtain distilled slag rich in selenium and precious metals, wherein the selenium content is about 15 to 20%, the tellurium content is 10 to 15%, the copper content is 20 to 27%, the silver content is 1 to 5%, the lead content is 1 to 4%, the sodium content is 8 to 15%, and the gold content is 5001 to 2000g/t, wherein the main phases of selenium and tellurium are Cu 2 Se、Cu 3 Se 2 And noble metal tellurides, in addition, sodium is present in the form of sodium chloride.
At present, selenium and tellurium are separated from selenium-containing materials and precious metals are enriched mainly by a pyrogenic process and a wet process, selenium recovered by the pyrogenic process is mainly recovered in flue gas by a sulfating roasting mode, tellurium is recovered in soda ash of a precious lead furnace, but harmful gases are generated, the environment is polluted greatly, the energy consumption is large, the production period is long, and the likeThe title is obtained. Hydrometallurgy is a mainstream method gradually replacing pyrometallurgy because it is relatively environment-friendly, low in energy consumption, low in cost and high in recovery rate of valuable metals. CN201510785877.0 discloses a NaOH compound H 2 O 2 And then the method of leaching alkaline slag by using acid solution is used for separating selenium and tellurium enriched noble metals, the leaching rate of selenium and tellurium can reach 85.91 percent and 96.32 percent, but an acid-alkali conversion process is needed. CN201910335008.6 discloses a method for recovering selenium from high tellurium-silver-selenium slag by vacuum distillation, but for the silver-gold-rich steamed selenium slag, the selenium-tellurium recovery rate is not high. CN201110408924.1 discloses an H 2 SO 4 Coordination H 2 O 2 The selenium leaching rate of the method for recovering selenium from the selenium-containing materials reaches 95-98 percent, but the leaching rate of selenium and tellurium is not high for the silver-gold-rich selenium steaming slag, and the reaction is violent and is difficult to control.
Aiming at the occurrence characteristics of selenium tellurium copper and noble metal in the selenium steaming slag, the method improves the leaching rate of selenium tellurium by matching oxygen pressure and hydrogen peroxide in a sulfuric acid system, realizes the separation of selenium tellurium copper and noble metal, keeps mild leaching and has easily controlled leaching process.
Disclosure of Invention
The invention aims to provide a method for leaching selenium, tellurium and copper and enriching noble metals from silver-gold-enriched selenium steaming slag, which comprises the following steps:
(1) Under the condition of existence of hydrogen peroxide and oxygen pressure, leaching the silver-gold-rich selenium steaming slag by adopting a sulfuric acid system, stirring and keeping the solution in a suspension state, so that selenium, tellurium and copper are dissolved in the sulfuric acid solution, and silver, gold and other noble metals and lead are remained in the leaching slag, thereby realizing the separation of selenium, tellurium and copper and noble metals;
(2) The leaching solution is further subjected to reduction and purification processes to recover selenium, tellurium and copper, and the leaching residues are subjected to reduction smelting to further recover precious metals and lead.
Preferably, in the step (1) of the invention, the silver-rich gold-evaporated selenium slag is crude selenium powder recovered from copper anode mud produced by copper smelting, and is subjected to a series of processes of closed smelting and vacuum distillation to obtain distilled selenium slag, wherein the content of selenium is about 15 to 20%, tellurium is 10 to 15%, copper is 20 to 27%, silver is 1 to 5%, lead is 1 to 4%, sodium is 8 to 15%, and gold is 5001 to 2000g/tWherein the main phase of selenium and tellurium is Cu 2 Se、Cu 3 Se 2 And noble metal tellurides, in addition, sodium is present in the form of sodium chloride.
Preferably, in the step (1) of the invention, the concentration of the sulfuric acid is controlled to be 3-4 mol/L, and the concentration of the hydrogen peroxide is controlled to be 35%; the addition amount is 11 to 13 times of the theoretical dosage, and the liquid-solid ratio is 17 to 1.
Preferably, in the step (1), the oxygen flow rate is 1 to 2L/min or the oxygen pressure is 1 to 10 atm, the stirring speed is 300rpm, and the reaction time is 1 to 3h.
The processes of reduction, purification, reduction smelting and the like in the step (2) of the invention are all conventional methods.
The principle of the invention is as follows:
Cu 2 Se、Cu 3 Se 2 and metal tellurides are substituted by H under acidic conditions 2 O 2 By oxidation to H 2 SeO 3 、H 2 TeO 3 And sulfate, so that the selenium tellurium copper is separated from the lead and the noble metal and enters the leaching solution; oxygen is introduced to not only oxidize Cu as an oxidant 2 Se、Cu 3 Se 2 And metal tellurides, and can suppress H under acidic conditions 2 O 2 Is decomposed to H 2 O 2 Better plays the role of the catalyst, thereby improving the recovery rate of the metal.
The invention has the following beneficial effects:
oxygen is introduced, the recovery rate of selenium and tellurium is increased, the leaching rates of selenium and tellurium are respectively increased by about 10% and 5% under normal pressure, the leaching rates of selenium and tellurium are respectively increased by about 20% and 15% under the pressurization condition, and the reaction intensity of silver-rich gold steamed selenium slag, hydrogen peroxide and sulfuric acid is reduced, so that the control is easy; sodium chloride exists in the silver-rich gold selenium steaming slag, reacts with silver to form silver chloride, and the silver chloride is remained in the slag to be enriched; the method has the advantages of simple operation, high leaching rate of selenium, tellurium and copper and high recovery rate of noble metals.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the scope of the present invention is not limited to the examples.
Example 1
A method for leaching and separating valuable metals from silver-gold-rich selenium steaming slag comprises the following specific steps: crushing 10g of silver-rich gold selenium steaming slag, grinding the silver-rich gold selenium steaming slag to 200-300 meshes, adding the silver-rich gold selenium steaming slag into 200mL of sulfuric acid mixed solution at 25 ℃ for leaching, wherein 129mL of H with the mass fraction of 35% is added 2 O 2 Introducing oxygen; controlling the concentration of sulfuric acid to be 3.5mol/L, the flow of oxygen to be 2L/min, the stirring speed to be 300rpm, and keeping the temperature of water bath to be 25 ℃ for leaching for 3h; carrying out vacuum filtration to separate solid from liquid, carrying out constant volume treatment on the pickle liquor to 500mL, sending the pickle liquor to the detection of element content, and calculating the leaching rate; and washing the acid leaching residue for three times, drying the acid leaching residue at 90 ℃ for 24 hours to detect the element phase, and calculating the residue rate. The leaching rate of the acid leaching solution with selenium as a main element is obtained through analysis and detection: 88.89% of selenium, 84.93% of tellurium and 89.81% of copper.
When other conditions are the same, under the condition of not introducing oxygen, the leaching rate of main elements is as follows: 77.83% of selenium, 78.84% of tellurium and 87.84% of copper.
Example 2
A method for leaching and separating valuable metals from silver-gold-rich selenium steaming slag comprises the following specific steps: crushing 11.8g of silver-rich gold selenium steaming slag which is ground to 200-300 meshes, adding 200mL of sulfuric acid mixed solution at 25 ℃ for leaching, wherein 137mL of H with 35% of mass fraction is added 2 O 2 Introducing oxygen; controlling the concentration of sulfuric acid to be 3mol/L, the flow of oxygen to be 1.5L/min, the stirring speed to be 300rpm, and keeping the temperature of water bath to be 25 ℃ for leaching for 1h; carrying out vacuum filtration to separate solid from liquid, carrying out constant volume of pickle liquor to 500mL, sending the pickle liquor to detect the content of elements, and calculating the leaching rate; washing the acid leaching residue for three times, drying the acid leaching residue at 90 ℃ for 24 hours to detect the element phase, and calculating the residue rate. The leaching rate of main elements is as follows: 85.43 percent of selenium, 83.52 percent of tellurium and 89.87 percent of copper.
When other conditions are the same, under the condition of not introducing oxygen, the leaching rate of main elements is as follows: 75.95% of selenium, 78.73% of tellurium and 85.56% of copper.
Example 3
A method for leaching and separating valuable metals from silver-gold-rich selenium steaming slag comprises the following specific steps: crushing 11.1g, grinding to 200-300 meshSteaming selenium slag rich in silver and gold, adding 200mL of sulfuric acid mixed solution at 25 ℃ for leaching, wherein 120mL of H with 35% of mass fraction is added 2 O 2 Introducing oxygen; controlling the concentration of sulfuric acid to be 4mol/L, the flow of oxygen to be 1L/min, the stirring speed to be 300rpm, and keeping the temperature of the water bath to be 25 ℃ for leaching for 2h; carrying out vacuum filtration to separate solid from liquid, carrying out constant volume of pickle liquor to 500mL, sending the pickle liquor to detect the content of elements, and calculating the leaching rate; washing the acid leaching residue for three times, drying the acid leaching residue at 90 ℃ for 24 hours to detect the element phase, and calculating the residue rate. The leaching rate of main elements is as follows: 85.98% of selenium, 81.80% of tellurium and 88.61% of copper.
When other conditions are the same, the leaching rate of the main elements is as follows under the condition of not introducing oxygen: 77.19% of selenium, 76.85% of tellurium and 87.64% of copper.
Example 4
A method for leaching and separating valuable metals from silver-gold-rich selenium steaming slag comprises the following specific steps: crushing 30g of silver-gold-rich selenium steaming slag, grinding the silver-gold-rich selenium steaming slag to 200-300 meshes, adding the silver-gold-rich selenium steaming slag into 600mL of sulfuric acid mixed solution at 25 ℃ for leaching, wherein 387mL of H with the mass fraction of 35% is added 2 O 2 Introducing oxygen; controlling the concentration of sulfuric acid to be 3.5mol/L, the pressure of oxygen to be 0.5Mpa (5 atmospheric pressures), the stirring speed to be 300rpm, and keeping the temperature of the water bath to be 25 ℃ for leaching for 3h; carrying out vacuum filtration to separate solid from liquid, carrying out constant volume treatment on the pickle liquor to 1000mL, sending the pickle liquor to the detection of element content, and calculating the leaching rate; washing the acid leaching residue for three times, drying the acid leaching residue at 90 ℃ for 24 hours to detect the element phase, and calculating the residue rate. The leaching rate of the acid leaching solution with selenium as a main element is obtained through analysis and detection: 93.97% of selenium, 99.83% of tellurium and 92.65% of copper.
When other conditions are the same, under the condition of not introducing oxygen, the leaching rate of main elements is as follows: 77.83% of selenium, 78.84% of tellurium and 87.84% of copper.
Example 5
A method for leaching and separating valuable metals from silver-gold-rich selenium steaming slag comprises the following specific steps: crushing 35.4g of silver-rich gold selenium steaming slag which is ground to 200-300 meshes, adding the silver-rich gold selenium steaming slag into 600mL of sulfuric acid mixed solution at 25 ℃ for leaching, wherein 411mL of H with 35% of mass fraction is added 2 O 2 Introducing oxygen; controlling the concentration of sulfuric acid to be 3mol/L, the oxygen pressure to be 1Mpa, the stirring speed to be 300rpm, and leaching for 1h; vacuum filtering to separate solid from liquidSeparating, diluting the pickle liquor to 1000mL in constant volume, sending the pickle liquor to detect the element content, and calculating the leaching rate; washing the acid leaching residue for three times, drying the acid leaching residue at 90 ℃ for 24 hours to detect the element phase, and calculating the residue rate. The leaching rate of main elements is as follows: 93.90% of selenium, 93.90% of tellurium and 90.14% of copper.
When other conditions are the same, under the condition of not introducing oxygen, the leaching rate of main elements is as follows: 75.95% of selenium, 78.73% of tellurium and 85.56% of copper.
Example 6
A method for leaching and separating valuable metals from silver-gold-rich selenium steaming slag comprises the following specific steps: 33.3g of silver-rich gold selenium steaming slag which is crushed and ground to 200-300 meshes is added into 600mL of sulfuric acid mixed solution for leaching at 25 ℃, and 360mL of H with 35 percent of mass fraction is added 2 O 2 Introducing oxygen; controlling the concentration of sulfuric acid to be 4mol/L, the pressure of oxygen to be 0.1Mpa, the stirring speed to be 300rpm, and leaching for 2h; carrying out vacuum filtration to separate solid from liquid, carrying out constant volume treatment on the pickle liquor to 1000mL, sending the pickle liquor to the detection of element content, and calculating the leaching rate; and washing the acid leaching residue for three times, drying the acid leaching residue at 90 ℃ for 24 hours to detect the element phase, and calculating the residue rate. The leaching rate of main elements is as follows: 91.98% of selenium, 93.57% of tellurium and 91.91% of copper.
When other conditions are the same, the leaching rate of the main elements is as follows under the condition of not introducing oxygen: 77.19% of selenium, 76.85% of tellurium and 87.64% of copper.
In conclusion, the recovery rates of selenium and tellurium are increased by introducing oxygen, and the recovery rates of selenium, tellurium and copper are further increased by pressurizing, and all the recovery rates are more than 90%.

Claims (4)

1. A method for leaching and separating valuable metals from silver-gold-rich selenium steaming slag is characterized by comprising the following steps:
(1) Under the condition of existence of hydrogen peroxide and oxygen pressure, leaching the silver-gold-rich selenium steaming slag by adopting a sulfuric acid system, stirring to keep the solution in a suspension state, dissolving selenium, tellurium and copper in the sulfuric acid solution, and remaining noble metals of silver, gold and lead in the leached slag to realize the separation of selenium, tellurium and copper from the noble metals;
(2) The leaching solution is further subjected to reduction and purification processes to recover selenium, tellurium and copper, and the leaching residues are subjected to reduction smelting to further recover precious metals and lead;
in the step (1), the oxygen flow is 1 to 2L/min or the oxygen pressure is 1 to 10 atmospheric pressures;
in the step (1), the mass percent concentration of the hydrogen peroxide is 35%, the addition amount is 11 to 13 times of the theoretical dosage, and the liquid-solid ratio is 17 to 1.
2. The method for separating valuable metals by leaching the silver-gold-rich selenium-steaming slag according to claim 1, which is characterized by comprising the following steps: the silver-gold-rich selenium steaming slag in the step (1) is crude selenium powder produced by recovering copper anode slime produced by copper smelting, and is subjected to a series of processes of closed smelting and vacuum distillation to obtain distilled selenium slag.
3. The method for separating valuable metals by leaching the silver-gold-rich selenium-steaming slag according to claim 1, which is characterized by comprising the following steps: in the step (1), the concentration of sulfuric acid is controlled to be 3 to 4mol/L.
4. The method for separating valuable metals by leaching the silver-gold-rich selenium-steaming slag according to claim 1, which is characterized by comprising the following steps: in the step (1), the stirring speed is 300rpm, and the reaction time is 1 to 3h.
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